Complex for preparing highly branched poly (4-methyl-1-pentene) material and preparation method thereof

The technology of a complex and trimethylaluminum is applied in the preparation of a complex of a highly branched poly-4-methyl-1-pentene material and the preparation field thereof, and can solve the problem of inability to catalyze the copolymerization of olefins and polar monomers, assist the The problem of expensive catalyst methylaluminoxane and high manufacturing cost

Inactive Publication Date: 2021-05-04
张洪胜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the production cost of metallocene catalysts or non-metallocene catalysts of the early transition metal system is high, and the cocatalyst methylaluminoxane (MAO) is expensive and used in large amounts, and the active center is easily deactivated by polar functional groups and cannot be catalyzed. Defects such as copolymerization of olefins and p

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  • Complex for preparing highly branched poly (4-methyl-1-pentene) material and preparation method thereof
  • Complex for preparing highly branched poly (4-methyl-1-pentene) material and preparation method thereof
  • Complex for preparing highly branched poly (4-methyl-1-pentene) material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] This embodiment provides a diimine ligand, and its synthesis method is as follows.

[0031] Under nitrogen atmosphere and room temperature, add 20mL of toluene, 2,6-dipropyl-4-methoxyaniline (12mmol) into a 100mL branch bottle, and then add 12mL of trimethylaluminum (1.0M, 12mmol); The reaction temperature was raised to 110°C, and after 2 hours of reaction, the reaction temperature was lowered to room temperature, and then acenaphthylquinone (5mmol) was added; at this time, the reaction system changed from colorless to deep red, and a large amount of heat was emitted; at 110°C, continue React for 6 hours, then lower the temperature to 0°C, and terminate the reaction system with 5% sodium hydroxide ice solution; extract the organic phase with ethyl acetate, and then use anhydrous MgSO 4 Dry and spin the solvent under reduced pressure to obtain an orange oil; the product is separated through a silica gel column, eluent (petroleum ether: ethyl acetate = 15:1); recrystalliz...

Embodiment 2

[0033] This example provides a diimine palladium complex, the synthesis method of which is as follows.

[0034] Under nitrogen protection, diimine ligand (0.5mmol), (COD)PdMeCl (0.6mmol) and 20mL of dichloromethane were added into a Schlenk bottle with a branch, and the reaction was stirred at room temperature for 12 hours, and then reduced at room temperature to The solvent was evaporated under pressure to about 5ml, and 20ml of n-hexane was added, at which point a large amount of precipitation occurred. Filter with G4 filter ball, wash the precipitate with 3×10 mL of n-hexane, and then vacuum-dry to obtain a yellow solid powder diimide palladium complex with a yield of 78.6%.

Embodiment 3

[0036] This embodiment provides a highly branched poly(4-methyl-1-pentene), the preparation method of which is as follows.

[0037] All the glass instruments and magnets used for stirring were dried in an oven (120°C), and all polymerization experiments were carried out under anhydrous and oxygen-free conditions. Under continuous vacuuming, bake a 250mL branched-mouthed round-bottom flask under an infrared lamp at 150°C for more than 1 hour to remove all moisture and air; replace it with nitrogen twice and then fill it with nitrogen to normal pressure; keep the water bath at 30 ℃, add metered amount of chlorobenzene, stir to dissolve and inject 2M monomer and 10 μmol diimine palladium complex dissolved in 2 mL of dichloromethane. Stop the reaction after polymerizing to 4h, use Et 3 After SiH terminated, it was precipitated in methanol. The precipitated polymer was dissolved in petroleum ether, separated by silica gel column, concentrated, and precipitated in methanol. The obt...

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Abstract

The invention discloses a complex for preparing a highly branched poly (4-methyl-1-pentene) material and a preparation method of the complex. When the diimine palladium complex is applied to 4-methyl-1-pentene polymerization, the reaction condition is mild, and the polymerization reaction does not need to be carried out under harsh anhydrous and anaerobic conditions; according to the present invention, the propyl group is introduced to the ortho-position of the imine nitrogen atom aromatic ring, so that the dynamic steric hindrance can be provided for the complex during the catalytic polymerization process so as to finely adjust the space environment of the Pd catalytic activity center, regulate the branching degree and the molecular weight of the polymer, and obtain the highly branched poly 4-methyl-1-pentene;.

Description

technical field [0001] The invention belongs to the field of polyolefin preparation, and in particular relates to a complex for preparing highly branched poly-4-methyl-1-pentene material and a preparation method thereof. Background technique [0002] Poly-4-methyl-1-pentene can be formed by injection molding, blow molding, extrusion molding and other methods. The main purpose is to manufacture medical equipment (such as syringes), physical and chemical laboratory equipment, special food utensils for electronic stoves, baking trays, release paper, heat-resistant wire coatings, etc. The monomer 4-methyl-1-pentene is obtained by dimerization of propylene, and then obtained by polymerization with a catalyst. [0003] In recent years, the research on using 4-methyl-1-pentene as a homopolymerization or comonomer mainly focuses on metallocene catalysts and non-metallocene catalysts of early transition metal systems. However, the production cost of metallocene catalysts or non-met...

Claims

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Application Information

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IPC IPC(8): C07F15/00C08F110/14C08F4/80
CPCC07F15/0066C08F110/14
Inventor 张洪胜
Owner 张洪胜
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